JP2010180458A - Method for forming oxide layer on aluminum surface and method for manufacturing semiconductor device - Google Patents
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本発明は、アルミニウム（Ａｌ）又はアルミニウム合金を、高濃度の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成すること、および半導体または極薄の酸化物（酸化シリコン）の被膜の形成された半導体の上に存するアルミニウム（Ａｌ）又はアルミニウム合金を、高濃度の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成することをそなえた半導体装置の製造方法に関する。 In the present invention, aluminum (Al) or an aluminum alloy is immersed in high-concentration nitric acid to form a production film of aluminum oxide (Al 2 O 3 ) on the surface of the aluminum or aluminum alloy, and a semiconductor or ultrathin film. Aluminum (Al) or an aluminum alloy existing on the semiconductor on which the oxide (silicon oxide) film is formed is immersed in high-concentration nitric acid, and aluminum oxide (Al 2 O 3) is formed on the surface of the aluminum or aluminum alloy. ) Of a semiconductor device having a formation film formed thereon.
アルミニウム（Ａｌ）又はアルミニウム合金は、通常、空気中に放置するだけで、表面に数ナノメートル（ｎｍ）の酸化物（自然酸化物とも呼ばれる）が形成されているが、多くの電子デバイス、とりわけ、半導体装置等の配線や電極部分にアルミニウム合金層を使用する半導体電子デバイスの場合、配線間間隔が微細化されるとともに配線間のリークが増大するという問題が発生しやすくなり、微細化の妨げとなっている。またアルミニウム電極上に良好な酸化アルミニウムが形成できれば、それを容量として用いることが可能となり、アナログ集積回路やガラス基板上の低温ポリシリコントランジスタ集積回路の微細化や高性能化が可能となる。一方、かかる半導体電子デバイスがプラスチックパッケージ中にカプセル封止されているときに生じる上記アルミニウム合金層の腐食を抑制することも、信頼性の重要な課題である。 Aluminum (Al) or an aluminum alloy usually has an oxide (also called a natural oxide) of several nanometers (nm) formed on the surface only by leaving it in the air. In the case of a semiconductor electronic device using an aluminum alloy layer for wiring and electrode parts of a semiconductor device or the like, the problem that the inter-wiring spacing is miniaturized and leakage between the wirings is liable to occur, preventing miniaturization. It has become. If good aluminum oxide can be formed on the aluminum electrode, it can be used as a capacitor, and the analog integrated circuit and the low-temperature polysilicon transistor integrated circuit on the glass substrate can be miniaturized and improved in performance. On the other hand, suppressing the corrosion of the aluminum alloy layer that occurs when the semiconductor electronic device is encapsulated in a plastic package is also an important reliability issue.
それに関して、一例として、アルミニウム−珪素（Ａｌ−Ｓｉ）合金の金属層上に非常に薄い不働体化ホスフェート層またはリン酸化フィルム生成して、同金属層が湿った雰囲気中で応力を受けたときに、同合金層の腐食／ヒドロキシル化作用に抗するのに有効な抑制手段にすることが知られ（特許文献１）、その過程の第1段階（工程１）で同金属層を濃度100％の硝酸に浸漬することも示されているが、この段階での硝酸処理は、次の第2段階（工程２）で少量のリン酸（Ｈ３ＰＯ４）を含む混合物中に浸漬して金属層をホスフェートフィルムで被覆する前処理であり、アルミニウム−ケイ素（Ａｌ−Ｓｉ）合金の金属層上に酸化アルミニウムのみの被膜を形成するものではない。 In that regard, as an example, when a very thin passivated phosphate layer or phosphorylated film is formed on a metal layer of an aluminum-silicon (Al-Si) alloy and the metal layer is stressed in a humid atmosphere In addition, it is known to be an effective suppression means for resisting the corrosion / hydroxylation action of the alloy layer (Patent Document 1), and the concentration of the metal layer is 100% in the first stage of the process (Process 1). In this stage, nitric acid treatment is performed by dipping in a mixture containing a small amount of phosphoric acid (H 3 PO 4 ) in the next second stage (step 2). This is a pretreatment for coating a layer with a phosphate film, and does not form an aluminum oxide-only coating on a metal layer of an aluminum-silicon (Al-Si) alloy.
また、近年、超高密度ＭＯＳデバイス等で、酸化アルミニウム（Ａｌ２Ｏ３）膜を半導体界面の応力付加層として利用するという試みもあり、電子材料として酸化アルミニウム（Ａｌ２Ｏ３）膜を半導体電子デバイスへ広く利用する場合の対応には、安定、かつその膜厚を十分に確保できる等、高いデバイス適応性のある，酸化アルミニウム膜およびその製造方法が望まれている。 In recent years, semiconductor ultra high density MOS devices and the like, are also attempts to use the aluminum oxide (Al 2 O 3) film as a stressing layer of semiconductor interface, the aluminum oxide (Al 2 O 3) film as electronic material In order to cope with a wide range of applications in electronic devices, an aluminum oxide film and a method for manufacturing the same that have high device adaptability, such as being stable and ensuring a sufficient film thickness, are desired.
本発明の主な目的は、アルミニウムまたはアルミニウム合金層に対して、自然酸化物ではなく、かつそれより厚い酸化アルミニウムの被膜を化学的に生成すること、および前記アルミニウム又はアルミニウム合金の表面に酸化アルミニウムの生成膜を形成することをそなえた半導体装置の製造方法を提供することにある。 The main object of the present invention is to chemically generate a coating of aluminum oxide that is not a natural oxide and thicker than that of an aluminum or aluminum alloy layer, and aluminum oxide on the surface of the aluminum or aluminum alloy. It is an object of the present invention to provide a method for manufacturing a semiconductor device, which is provided with the formation of the above-described formed film.
本発明は、アルミニウム（Ａｌ）又はアルミニウム合金を、硝酸，好ましくは濃度４０〜９９ｗｔ％の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成することを特徴とする酸化アルミニウム被膜の形成方法である。 In the present invention, aluminum (Al) or an aluminum alloy is immersed in nitric acid, preferably nitric acid having a concentration of 40 to 99 wt%, to form a production film of aluminum oxide (Al 2 O 3 ) on the surface of the aluminum or aluminum alloy. This is a method for forming an aluminum oxide film.
本発明は、４０℃未満，たとえば室温で、濃度４０〜９９ｗｔ％の範囲の所定の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に厚さが通常の自然酸化膜の厚さを超える２ナノメートル（ｎｍ）以上の酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成することを特徴とする酸化アルミニウム被膜の形成方法である。 The present invention is to immerse in a predetermined nitric acid having a concentration of 40 to 99 wt% at a temperature of less than 40 ° C., for example, room temperature, so that the thickness of the surface of the aluminum or aluminum alloy exceeds 2 nm. A method of forming an aluminum oxide film, comprising forming a film of aluminum oxide (Al 2 O 3 ) having a thickness of at least meters (nm).
さらに、本発明は、半導体上、もしくは極薄の酸化物被膜を有する半導体上にアルミニウム（Ａｌ）又はアルミニウム合金を、４０℃未満，たとえば室温で、硝酸，好ましくは濃度４０〜９９ｗｔ％の範囲の所定の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に厚さが通常の自然酸化膜の厚さを超える２ナノメートル（ｎｍ）以上の酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成することをそなえた半導体装置の製造方法である。 Furthermore, the present invention provides a method of applying aluminum (Al) or an aluminum alloy on a semiconductor or on a semiconductor having an ultra-thin oxide film at a temperature below 40 ° C., for example, room temperature, nitric acid, preferably in the range of 40 to 99 wt%. A film of aluminum oxide (Al 2 O 3 ) having a thickness of 2 nanometers (nm) or more exceeding the thickness of a normal natural oxide film is formed on the surface of the aluminum or aluminum alloy by immersing in predetermined nitric acid. This is a method of manufacturing a semiconductor device.
本発明によると、アルミニウム（Ａｌ）表面、または基体上に形成したアルミニウム（Ａｌ）成膜を、硝酸，好ましくは濃度４０〜９９ｗｔ％の範囲の所定の硝酸に浸して、厚さが通常の自然酸化膜の厚さを超える２ナノメートル（ｎｍ）以上の酸化アルミニウム（Ａｌ２Ｏ３）被膜を形成することができ、この酸化アルミニウム（Ａｌ２Ｏ３）被膜は、他金属等の不純物を含まず、高絶縁性の誘電体層として、電気的諸特性に優れており、電子デバイスの高性能な機能要素に利用可能である。 According to the present invention, an aluminum (Al) film formed on an aluminum (Al) surface or a substrate is immersed in nitric acid, preferably a predetermined nitric acid having a concentration in the range of 40 to 99 wt%, so that the thickness is normal natural. An aluminum oxide (Al 2 O 3 ) film having a thickness of 2 nanometers (nm) or more exceeding the thickness of the oxide film can be formed. This aluminum oxide (Al 2 O 3 ) film contains impurities such as other metals. As a highly insulating dielectric layer, it has excellent electrical characteristics and can be used for high-performance functional elements of electronic devices.
本発明によると、半導体の上に存するアルミニウム（Ａｌ）又はアルミニウム合金を、４０℃未満，たとえば室温で、硝酸，好ましくは濃度４０〜９９ｗｔ％の範囲の所定の硝酸に浸して、前記アルミニウム又はアルミニウム合金の表面に厚さが通常の自然酸化膜の厚さを超える２ナノメートル（ｎｍ）以上，望ましくは、１０ナノメートル（ｎｍ）以上の酸化アルミニウム（Ａｌ２Ｏ３）の生成膜を形成することが可能である。 According to the present invention, aluminum (Al) or an aluminum alloy existing on a semiconductor is immersed in nitric acid, preferably a predetermined nitric acid having a concentration in the range of 40 to 99 wt% at less than 40 ° C., for example, room temperature, to obtain the aluminum or aluminum. A formed film of aluminum oxide (Al 2 O 3 ) having a thickness of 2 nanometers (nm) or more, preferably 10 nanometers (nm) or more, exceeding the thickness of a normal natural oxide film is formed on the surface of the alloy. It is possible.
シリコンウェーハ上にアルミニウム合金（Ａｌ中に１％のＳｉを含む）で厚さ２００ｎｍの成膜１を設け、同成膜１を室温（２５℃）で所定濃度の硝酸に浸漬して、その後、超純水で洗浄し、乾燥した。 A film 1 having a thickness of 200 nm is provided on a silicon wafer with an aluminum alloy (containing 1% Si in Al), and the film 1 is immersed in nitric acid at a predetermined concentration at room temperature (25 ° C.). Washed with ultrapure water and dried.
図１は、シリコン基板上に成膜したアルミニウム薄膜の試料を濃度７０ｗｔ％の硝酸に室温で浸漬して得られた，Ａｌ２Ｏ３／Ａｌ構造のＸＰＳスペクトル特性図である。硝酸酸化処理を全く行わない試料面にも自然酸化のＡｌ２Ｏ３膜が形成されているが、浸漬時間経過とともに、表面部のＡｌ２Ｏ３／Ａｌ構造が順次、Ａｌ２Ｏ３のピーク増大へと、表面の変化が観られ、Ａｌ２Ｏ３の被膜の形成が進むことを示している。また、ＸＰＳスペクトル特性図から推定される酸化アルミニウムの膜厚は、３．３ｎｍ（０分）、５．４ｎｍ（５分）、５．８ｎｍ（１０分），８．１ｎｍ（２０分），８．７ｎｍ（３０分）、１１．７ｎｍ（４０分），１２．５ｎｍ（５０分）および１２．９ｎｍ（６０分）であり、いずれの場合も、表面の鏡面性は保たれていた。 FIG. 1 is an XPS spectral characteristic diagram of an Al 2 O 3 / Al structure obtained by immersing a sample of an aluminum thin film formed on a silicon substrate in nitric acid having a concentration of 70 wt% at room temperature. A naturally oxidized Al 2 O 3 film is also formed on the sample surface where no nitric acid oxidation treatment is performed, but the Al 2 O 3 / Al structure on the surface portion sequentially shows the peak of Al 2 O 3 as the immersion time elapses. As it increases, a change in the surface is observed, indicating that the formation of the Al 2 O 3 coating proceeds. The film thickness of the aluminum oxide estimated from the XPS spectral characteristic diagram is 3.3 nm (0 minute), 5.4 nm (5 minutes), 5.8 nm (10 minutes), 8.1 nm (20 minutes), 8 It was 0.7 nm (30 minutes), 11.7 nm (40 minutes), 12.5 nm (50 minutes) and 12.9 nm (60 minutes), and in all cases, the specularity of the surface was maintained.
図2は、濃度７０ｗｔ％の硝酸に室温で２０分間浸漬して得られた酸化膜の透過電子顕微鏡（ＴＥＭ）による観察断面図であり、アルミニウム（Ａｌ）成膜１上の酸化アルミニウム（Ａｌ２Ｏ３）被膜２の厚み（図中の矢印先端間寸法で表示）は約２０ｎｍであった。なお、図示の試料構造は、酸化アルミニウム（Ａｌ２Ｏ３）被膜２の表面には樹脂材３を設けてＴＥＭ観察用に試料形成したものである。このＴＥＭ観察によると、酸化アルミニウム（Ａｌ２Ｏ３）被膜の均一性も良いことが分かる。 FIG. 2 is a cross-sectional view of an oxide film obtained by immersing in nitric acid having a concentration of 70 wt% at room temperature for 20 minutes by a transmission electron microscope (TEM), and shows aluminum oxide (Al 2 ) on the aluminum (Al) film 1. The thickness of the O 3 ) coating 2 (indicated by the dimension between the tips of the arrows in the figure) was about 20 nm. In the illustrated sample structure, a resin material 3 is provided on the surface of an aluminum oxide (Al 2 O 3 ) coating 2 and a sample is formed for TEM observation. According to this TEM observation, it can be seen that the uniformity of the aluminum oxide (Al 2 O 3 ) film is also good.
図3は、代表的な電気特性として例示の電圧−電流特性図であり、濃度７０ｗｔ％の硝酸に室温で２０分間浸漬して得られた酸化膜の生成直後の特性と、未処理サンプルとして、硝酸酸化処理を全く行わないリファレンス試料で表面には厚さ約３．５ｎｍの自然酸化膜が形成されているものとを対比して示した。 FIG. 3 is an exemplary voltage-current characteristic diagram as typical electrical characteristics. The characteristics immediately after the formation of an oxide film obtained by immersing in nitric acid having a concentration of 70 wt% at room temperature for 20 minutes, and an untreated sample, This is shown in comparison with a reference sample which is not subjected to nitric acid oxidation treatment and has a natural oxide film having a thickness of about 3.5 nm on the surface.
濃度７０ｗｔ％の硝酸に室温で２０分間浸漬して得られた酸化膜について、電気容量（Ｃ）の測定結果から、この酸化膜の比誘電率は６．９と見積られた。この値は、従来から知られるバルクＡｌ２Ｏ３被膜の比誘電率（約１０）と比べると少し小である。この生成酸化アルミニウム膜をＴＥＭとＳＥＭで観察したところ、ナノ構造の細孔が存在しているものが観察された。これが比誘電率のやや小さい理由と考えられる。 With respect to the oxide film obtained by immersing in nitric acid having a concentration of 70 wt% at room temperature for 20 minutes, the dielectric constant of the oxide film was estimated to be 6.9 from the measurement result of the electric capacity (C). This value is slightly smaller than the relative dielectric constant (about 10) of the conventionally known bulk Al 2 O 3 coating. When this generated aluminum oxide film was observed with TEM and SEM, it was observed that nanostructured pores were present. This is considered to be the reason why the relative permittivity is slightly small.
次に、実施例1と同形の試料面を濃度の異なる硝酸（硝酸濃度９８ｗｔ％，６１ｗｔ%，４０ｗｔ%）に各々１０〜２０分間浸して得た酸化膜の表面について、ＴＥＭおよびＸＰＳの結果から評価したところ、生成された酸化膜は平均的な膜厚、および表面の均一性並びに鏡面性に関して、いずれも実施例１の場合と同等で、概ね良好に保たれていた。ただ、濃度９８ｗｔ％の硝酸の場合には、濃度７０ｗｔ％の硝酸の場合に比べて、誘電率が少し大であった。ＴＥＭとＳＥＭで観察したところ、細孔構造はほとんど観察されなかった。 Next, from the results of TEM and XPS, the surface of the oxide film obtained by immersing the sample surface of the same shape as in Example 1 in nitric acid having different concentrations (nitric acid concentration 98 wt%, 61 wt%, 40 wt%) for 10 to 20 minutes, respectively. As a result of evaluation, the generated oxide film was almost the same as in Example 1 with respect to the average film thickness, surface uniformity and specularity, and was generally kept good. However, in the case of nitric acid having a concentration of 98 wt%, the dielectric constant was slightly larger than in the case of nitric acid having a concentration of 70 wt%. When observed with TEM and SEM, the pore structure was hardly observed.
以上、シリコン基板上のアルミニウム膜を用いた実験について述べたが、半導体として炭化ケイ素（ＳｉＣ）や化合物半導体またはガラス基板上のポリシリコン膜や非晶質シリコン膜上に形成されたアルミニウム膜にも適用可能である。シリコン等の半導体上に予め、硝酸酸化法を用いて、極薄の酸化物（酸化シリコン）の被膜を形成したものを用いても良い。この場合、酸化アルミニウム膜と酸化シリコン膜のスタック構造が可能となり、高性能なトランジスタ用ゲート酸化膜や不揮発性メモリに適用可能である。 As mentioned above, although the experiment using the aluminum film on the silicon substrate has been described, the silicon film (SiC) or compound semiconductor as a semiconductor or the aluminum film formed on the polysilicon film or the amorphous silicon film on the glass substrate is also described. Applicable. A semiconductor in which a very thin oxide (silicon oxide) film is previously formed on a semiconductor such as silicon by nitric acid oxidation may be used. In this case, a stack structure of an aluminum oxide film and a silicon oxide film is possible, and it can be applied to a high-performance gate oxide film for a transistor or a nonvolatile memory.
本発明は、合金を含むアルミニウム（Ａｌ）表面、または基体上に形成したアルミニウム（Ａｌ）成膜上に非常に薄い高絶縁性誘電体ないしは酸化アルミニウムの被膜を生成すること、およびかかる高絶縁性誘電体ないしは酸化アルミニウムの被膜を形成する表面処理により、合金を含むアルミニウム表面への酸化アルミニウムの被膜形成を利用する固体の電子デバイスおよびその製造方法に適用できるほか、高絶縁性誘電体ないしは酸化アルミニウムの被膜を電気エネルギー源、たとえば水素等の素材を蓄積する媒体とすることや高容量の電気容量素子に利用可能である。また、ナノ細孔の生じる酸化アルミニウムはメモリ容量や不揮発性メモリの容量絶縁膜に用いることも可能である。 The present invention produces a very thin highly insulating dielectric or aluminum oxide film on an aluminum (Al) surface containing an alloy or on an aluminum (Al) film formed on a substrate, and such high insulation. It can be applied to solid electronic devices using aluminum oxide film formation on aluminum surfaces including alloys by surface treatment to form a dielectric or aluminum oxide film, and a manufacturing method thereof, as well as a highly insulating dielectric or aluminum oxide This film can be used as an electric energy source, for example, a medium for storing a material such as hydrogen, or a high capacity electric capacity element. In addition, aluminum oxide in which nanopores are formed can be used for a memory capacitor or a capacitor insulating film of a nonvolatile memory.
１ アルミニウム（Ａｌ）成膜
２ 酸化アルミニウム（Ａｌ２Ｏ３）被膜
３ 樹脂材
1 Aluminum (Al) film formation 2 Aluminum oxide (Al 2 O 3 ) coating 3 Resin material
Claims (4)
Aluminum or an aluminum alloy existing on a semiconductor or a semiconductor on which an oxide film is formed is immersed in nitric acid having a concentration of 40 to 99% to form a production film of aluminum oxide on the surface of the aluminum or aluminum alloy. A method of manufacturing a semiconductor device.
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